CN111375358B - Method for improving gel efficiency in production of silicon-based aerogel composite material - Google Patents
Method for improving gel efficiency in production of silicon-based aerogel composite material Download PDFInfo
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- CN111375358B CN111375358B CN202010270839.2A CN202010270839A CN111375358B CN 111375358 B CN111375358 B CN 111375358B CN 202010270839 A CN202010270839 A CN 202010270839A CN 111375358 B CN111375358 B CN 111375358B
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- sol
- gel
- liquid
- flow
- based aerogel
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 46
- 239000010703 silicon Substances 0.000 title claims abstract description 46
- 239000004964 aerogel Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 238000007598 dipping method Methods 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000004064 recycling Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 2
- 239000007924 injection Substances 0.000 claims 2
- 239000002699 waste material Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
Abstract
The invention discloses a method for improving gel efficiency in the production of silicon-based aerogel composite materials, wherein a liquid silicon source and a liquid catalyst adopt flow control units to respectively and accurately control the flow of the liquid silicon source and the liquid catalyst, and realize automatic control through flow ratio interlocking; the invention not only improves the gel efficiency of the silicon-based aerogel composite material, but also effectively controls the generation of waste rubber at the bottom of the gum dipping box, avoids the blockage of the gum dipping box by the waste rubber, and improves the utilization of raw materials. Meanwhile, the flow of the liquid silicon source and the flow of the liquid catalyst are accurately and automatically controlled in an interlocking way, so that the gel speed is favorably controlled, and the normal continuous production of the gel is ensured.
Description
Technical Field
The invention relates to a gel reaction method in the production of silicon-based aerogel composite materials.
Background
In the production process of the silicon-based aerogel composite material, the gel reaction is an important operation step, and the production quality, the production efficiency and the production cost of the silicon-based aerogel composite material are related.
Currently, in the production of known silicon-based aerogel composite materials, the device and method for the gel reaction are as follows: the liquid silicon source and the liquid catalyst are fed directly into the mixer 03, respectively. Mixing in a mixer to form a sol, and then coating the sol on the surface of a solid substrate in a bottom flat dipping box 04 at a certain flow rate. The solid substrate is soaked by the liquid sol, and gel reaction is carried out in the solid substrate framework to generate the silicon-based aerogel composite material.
The known gel reaction in the production of silicon-based aerogel composite materials can not be controlled and regulated in proportion by the flow of a liquid silicon source and a liquid catalyst, and the liquid silicon source and the liquid catalyst are directly coated on the surface of a solid substrate in a bottom flat dipping box after being mixed in a mixer. The production process can generate excessive gel, so that the linear motion of the solid base material in the gum dipping box is influenced, and the uniform distribution of the sol in the solid base material is influenced, so that the product quality of the silicon-based aerogel composite material is influenced. Excessive sol is settled to the bottom of the gum dipping box, waste gum at the bottom of the gum dipping box is generated, the gum dipping box is blocked by the waste gum, the gum dipping box needs to be cleaned regularly, the gel speed is not controlled, normal continuous production of gel cannot be ensured, and meanwhile, the effective utilization of raw materials is reduced.
The known gel process flow of the silicon-based aerogel composite material is shown in figure 1.
Disclosure of Invention
The invention aims to provide a method for improving gel efficiency in the production of a silicon-based aerogel composite material, which not only improves the gel efficiency of the silicon-based aerogel composite material; meanwhile, the flows of the raw material liquid silicon source and the liquid catalyst realize accurate interlocking automatic control, which is beneficial to controlling the gel speed and ensuring normal continuous production.
The technical scheme adopted for solving the technical problems is as follows: a method for improving gel efficiency in the production of silicon-based aerogel composite materials is characterized in that a liquid silicon source and a liquid catalyst adopt flow control units to accurately control the flow respectively, and automatic control is realized through flow ratio interlocking; fully mixing the silicon source liquid and the catalyst liquid in a jet mixer, uniformly jetting the mixture on the surface of a solid substrate of a gum dipping box through a primary gel distributor, and performing gel reaction on a substrate framework by sol to generate a silicon-based aerogel composite material; and (3) the excessive sol is settled to the lower part of the dipping box with the gradient at the bottom, enters a recycling sol pressurizing unit, enters a recycling sol sprayer after being pressurized, is sprayed out from a secondary gel distributor, and performs secondary gel reaction in a solid substrate gap of the dipping box.
The invention has the following effects:
the invention can effectively improve the gel efficiency of the silicon-based aerogel composite material; and effectively control the waste rubber production of gum dipping box bottom, avoid the gum dipping box of waste rubber jam, maintain the rectilinear motion of solid substrate at the gum dipping box, reduced the work of regular clearance gum dipping box, guarantee the normal serialization production of gel. Meanwhile, the utilization rate of raw materials is improved by effectively utilizing the secondary gel of the recovered sol.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings used in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without any inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a known silica-based aerogel composite gel process.
Fig. 2 is a process flow diagram of the present invention.
The reference numerals illustrate a 01 liquid silicon source flow control unit, a 02 liquid catalyst flow control unit, a 03 mixer, a 04 gum dipping box, a 05 recovery sol pressurizing unit, a 06 recovery sol injector, a 07 interlocking unit, a 08 primary gel distributor and a 09 secondary gel distributor.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by a person of ordinary skill in the art based on the examples of the invention without any inventive effort, are within the scope of the invention.
The invention is embodied in three aspects: (1) The flow control units are adopted for the liquid silicon source and the liquid catalyst to precisely control the flow respectively, and automatic control is realized through flow ratio interlocking; (2) The silicon source liquid and the catalyst liquid are fully mixed in a jet mixer, then are evenly sprayed on the surface of a solid substrate of a gum dipping box through a primary gel distributor at a certain flow rate, so that the full penetration of the solid substrate is ensured, and the sol carries out gel reaction on a substrate framework to generate a silicon-based aerogel composite material; (3) And (3) depositing excessive sol at the bottom of the dipping box, entering a recycling sol pressurizing unit, pressurizing, entering a recycling sol sprayer, spraying the recycling sol into a solid substrate gap of the dipping box at a certain speed through a secondary gel distributor, and performing secondary gel reaction.
The invention, as shown in figure 2, comprises the following steps:
step 1, a liquid silicon source enters the jet mixer 03 through a liquid silicon source flow control unit 01, a flow signal is transmitted to an interlocking unit 07, calculation is carried out according to a set ratio, a flow signal of the liquid catalyst is output to a liquid catalyst flow control unit 02, and the liquid catalyst flow control unit receives the signal to control the flow of the liquid catalyst to enter the jet mixer 03. The volume flow ratio of the silicon source to the catalyst is 5:1-30:1, preferably 8:1-20:1.
Step 2, after the liquid silicon source and the liquid catalyst enter the jet mixer 03, the jet mixer adopts a static mixer, preferably a tubular jet mixer; the sol is formed by fully mixing in a jet mixer 03, and then the sol is sprayed from a primary gel distributor 08 at a certain flow rate, and uniformly sprayed on the surface of a solid substrate in a bottom slope gum dipping box 04, wherein the spraying flow rate is 0.5-4 m/s, preferably 0.8-2.5 m/s.
And 3, fully soaking the solid substrate by the liquid sol, performing a gel reaction in the solid substrate skeleton to generate a silicon-based aerogel composite material, controlling the starting frequency of a recovery sol pressurizing unit 05 through the liquid level of the bottom surface gradient dipping box 04, and recovering the sol at the bottom of the bottom surface gradient dipping box 04, wherein the starting frequency is 1-15 min/time, preferably 3-10 min/time, so as to prevent the sol from being gel into solid at the bottom of the bottom surface gradient dipping box 04. Meanwhile, the bottom plate of the bottom surface gradient gum dipping box 04 adopts a certain gradient slope direction recycling sol pressurizing unit 05, and the gradient value is 1-15%, preferably 3-10%; the reclaimed sol pressurizing unit 05 is in a form of no-retention liquid, and is preferably driven by a gas source.
And 4, feeding the recovered sol into a recovered sol sprayer 06, conveying the recovered sol from the recovered sol sprayer 06 to a secondary gel distributor 09, spraying the recovered sol from an outlet of the secondary gel distributor at a certain flow rate of 0.5-3 m/s, preferably 0.8-2 m/s, and finishing secondary gel in a solid substrate gap to improve the gel efficiency.
By the method, the gel efficiency of the silicon-based aerogel composite material is improved, waste rubber at the bottom of the gum dipping box is effectively controlled, the gum dipping box is prevented from being blocked by waste rubber, the linear motion of a solid substrate in the gum dipping box is prevented, the work of cleaning the gum dipping box regularly is reduced, and the normal continuous production of gel is ensured. Meanwhile, the flow of the raw material liquid silicon source and the flow of the liquid catalyst are accurately and automatically controlled, the gel speed is favorably controlled, the product quality is ensured, and the utilization rate of the raw material is improved.
It should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiment, it will be apparent to those skilled in the art that modifications may be made to the technical solution described in the foregoing embodiment, or that equivalents may be substituted for part of the technical features thereof.
Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for improving gel efficiency in the production of silicon-based aerogel composite materials is characterized in that a liquid silicon source and a liquid catalyst adopt flow control units to accurately control the flow respectively, and automatic control is realized through flow ratio interlocking; fully mixing the silicon source liquid and the catalyst liquid in a jet mixer, uniformly jetting the mixture on the surface of a solid substrate of a bottom slope gum dipping box through a primary gel distributor, and performing gel reaction on a solid substrate framework by sol to generate a silicon-based aerogel composite material; the excessive sol is settled to the bottom of the bottom slope dipping box, enters a recycling sol pressurizing unit, enters a recycling sol injector after being pressurized, is sprayed out of a secondary gel distributor, and performs secondary gel reaction in a solid substrate gap of the bottom slope dipping box;
the method specifically comprises the following steps:
step 1, a liquid silicon source enters an injection mixer through a liquid silicon source flow control unit, a flow signal is transmitted to an interlocking unit, calculation is carried out according to a set ratio, a flow signal of a liquid catalyst is output to a liquid catalyst flow control unit, the liquid catalyst flow control unit receives the signal, and the flow of the liquid catalyst is controlled to enter the injection mixer, wherein the volume flow ratio of the silicon source to the catalyst is 8:1-20:1;
step 2, after the liquid silicon source and the liquid catalyst enter a jet mixer, fully mixing in the jet mixer to form sol, then spraying the sol from a primary gel distributor at a certain flow rate, and uniformly spraying the sol on the surface of a solid substrate in a bottom slope gum dipping box;
step 3, fully soaking a solid substrate by liquid sol, performing a gel reaction in a solid substrate framework to generate a silicon-based aerogel composite material, controlling a sol recovery pressurizing unit to start frequency through the liquid level of a bottom surface gradient dipping box, recovering sol at the bottom of the bottom surface gradient dipping box, preventing the sol from being gelled into solid at the bottom of the bottom surface gradient dipping box, and simultaneously, adopting a certain gradient slope to recover the sol pressurizing unit on the bottom plate of the bottom surface gradient dipping box; wherein, the starting frequency of the pressurizing unit for recycling the sol is controlled to be 3-10 min/time; the reclaimed sol pressurizing unit is driven by an air source in a form of no reserved liquid; the value of the gradient is 1% -15%;
and 4, feeding the recovered sol into a recovered sol injector, conveying the recovered sol from the recovered sol injector to a secondary gel distributor, and spraying the recovered sol from an outlet of the secondary gel distributor at a certain flow rate to complete secondary gel in a solid substrate gap, thereby improving the gel efficiency.
2. The method for improving gel efficiency in the production of silica-based aerogel composites according to claim 1, wherein: the spraying flow rate of the sol sprayed by the primary gel distributor in the step 2 is 0.5-4 m/s.
3. The method for improving gel efficiency in the production of silica-based aerogel composites according to claim 1, wherein: the spraying flow rate of the primary gel distributor spraying sol in the step 2 is 0.8-2.5 m/s.
4. The method for improving gel efficiency in the production of silica-based aerogel composites according to claim 1, wherein: the gradient value described in the step 3 is 3% -10%.
5. The method for improving gel efficiency in the production of silica-based aerogel composites according to claim 1, wherein: the outlet of the secondary gel distributor described in the step 4 is sprayed out at a certain flow rate, and the flow rate is 0.5-3 m/s.
6. The method for improving gel efficiency in the production of silica-based aerogel composites according to claim 1, wherein: the outlet of the secondary gel distributor described in the step 4 is sprayed out at a certain flow rate, and the flow rate is 0.8-2 m/s.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010270839.2A CN111375358B (en) | 2020-04-08 | 2020-04-08 | Method for improving gel efficiency in production of silicon-based aerogel composite material |
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| CN202010270839.2A CN111375358B (en) | 2020-04-08 | 2020-04-08 | Method for improving gel efficiency in production of silicon-based aerogel composite material |
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| CN111375358A CN111375358A (en) | 2020-07-07 |
| CN111375358B true CN111375358B (en) | 2024-01-23 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011190136A (en) * | 2010-03-12 | 2011-09-29 | Asahi Kagaku Kk | Apparatus for manufacturing aerogel sheet |
| KR20120043329A (en) * | 2010-10-26 | 2012-05-04 | 엠파워(주) | Aerogel mat and aerogel mat manufacturing method using porous silica aerogel powder |
| KR101506096B1 (en) * | 2013-11-08 | 2015-03-25 | 지오스 에어로겔 리미티드 | Device and method for producing insulation textile impregnated aerogel using layer by layer type |
| CN105271403A (en) * | 2015-11-23 | 2016-01-27 | 哈尔滨工业大学 | Method for preparing zirconium oxide aerogel through combination of secondary gelling method and ambient-pressure drying |
| KR20170096514A (en) * | 2016-02-16 | 2017-08-24 | 주식회사 엘지화학 | Preparation method and apparatus of aerogel sheet |
| CN110483004A (en) * | 2019-09-10 | 2019-11-22 | 航天海鹰(镇江)特种材料有限公司 | A kind of aeroge preparation method that glue recycles |
| CN110775980A (en) * | 2019-11-27 | 2020-02-11 | 鑫创新材料科技(徐州)有限公司 | Efficient preparation method and application of aerogel |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060084707A1 (en) * | 2004-10-15 | 2006-04-20 | Aspen Aerogels, Inc. | Methods for manufacture of aerogels |
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2020
- 2020-04-08 CN CN202010270839.2A patent/CN111375358B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011190136A (en) * | 2010-03-12 | 2011-09-29 | Asahi Kagaku Kk | Apparatus for manufacturing aerogel sheet |
| KR20120043329A (en) * | 2010-10-26 | 2012-05-04 | 엠파워(주) | Aerogel mat and aerogel mat manufacturing method using porous silica aerogel powder |
| KR101506096B1 (en) * | 2013-11-08 | 2015-03-25 | 지오스 에어로겔 리미티드 | Device and method for producing insulation textile impregnated aerogel using layer by layer type |
| CN105271403A (en) * | 2015-11-23 | 2016-01-27 | 哈尔滨工业大学 | Method for preparing zirconium oxide aerogel through combination of secondary gelling method and ambient-pressure drying |
| KR20170096514A (en) * | 2016-02-16 | 2017-08-24 | 주식회사 엘지화학 | Preparation method and apparatus of aerogel sheet |
| CN110483004A (en) * | 2019-09-10 | 2019-11-22 | 航天海鹰(镇江)特种材料有限公司 | A kind of aeroge preparation method that glue recycles |
| CN110775980A (en) * | 2019-11-27 | 2020-02-11 | 鑫创新材料科技(徐州)有限公司 | Efficient preparation method and application of aerogel |
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| CN111375358A (en) | 2020-07-07 |
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